metals
Article
Comparison of Corrosion Resistance of the AA2524-T3 and
the AA2024-T3
Fernanda Martins Queiroz 1 , Maysa Terada 2, *, Aline F. Santos Bugarin 3 , Hercílio Gomes de Melo 4
and Isolda Costa 3






Citation: Queiroz, F.M.; Terada, M.;
Bugarin, A.F.S.; de Melo, H.G.; Costa,
I. Comparison of Corrosion
Resistance of the AA2524-T3 and the
AA2024-T3. Metals 2021, 11, 980.
https://doi.org/10.3390/met11060980
Academic Editor: Gilbert Henaff
Received: 6 May 2021
Accepted: 15 June 2021
Published: 19 June 2021
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Attribution (CC BY) license (https://
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4.0/).
Metals 2021, 11, 980. https://doi.org/10.3390/met11060980
1 Escola e Faculdade de Tecnologia SENAI Suiço-Brasileira “Paulo Ernesto Tolle”, Av. Bento Branco de
Andrade Filho, 379, São Paulo 04757-000, Brazil; mq_fernanda@yahoo.com.br
2 Instituto SENAI de Inovação em Manufatura Avançada e Microfabricação, Av. Bento Branco de Andrade
Filho, 379, São Paulo 04757-000, Brazil
3 IPEN, Instituto de Pesquisas Energéticas e Nucleares, Av. Prof. Lineu Prestes, 2242,
São Paulo 05508-000, Brazil; afbugarin@usp.br (A.F.S.B.); icosta@ipen.br (I.C.)
4 Escola Politécnica da University de São Paulo, Departament de Engenharia Metalúrgica e de Materiais, Av.
Prof. Mello de Moraes, 2463, São Paulo 05508-030, Brazil; hgdemelo@usp.br
* Correspondence: maysaterada@uol.com.br
Abstract: The 2XXX Al alloys are characterized by their superior mechanical properties resulting
from alloying elements and precipitation hardening treatments. The AA2524-T3 alloy was developed
to replace the AA2024-T3 alloy in the aerospace industry. However, both alloys present many
intermetallic particles (IMCs) in their microstructure, and this is the main reason for their high
susceptibility to localized corrosion (such as pitting and stress corrosion cracking). Despite the
similarities between these alloys (e.g., chemical composition and type of intermetallics) the literature
comparing their properties is scarce and focuses mainly on their mechanical properties, not their
corrosion resistances. In this investigation, the corrosion resistance of the AA2524-T3 alloy was
compared to the AA2024-T3 alloy. The microstructure of both alloys was analyzed by Scanning
Electron Microscopy before and after immersion in the test electrolyte, and the number and area
fraction of intermetallics of each alloy was determined. The corrosion resistance of both alloys was
monitored as a function of exposure time by electrochemical impedance spectroscopy and the results
were fitted using electrical equivalent circuits. The AA2524-T3 alloy presented not only higher
impedance values but also less corroded areas than the AA2024-T3 alloy.
Keywords: 2XXX aluminium alloys; intermetallics; aircraft industry; corrosion
1. Introduction
The 2XXX Al alloys are largely used in the aircraft industry due to their superior
mechanical properties resulting from alloying elements addition, mainly Cu and Mg, and
precipitation hardening treatments. The AA2524-T3 alloy is a relatively new alloy (formerly
known as C188-T3) developed by ALCOA to replace the AA2024-T3 alloy in fuselage skins.
It is currently used in the Boeing 777 aircraft [1,2]. It presents high damage-tolerance
and excellent fatigue properties [1]. However, both the AA2024-T3 and AA2524-T3 alloys
possess a large amount of intermetallic particles (IMCs) in their microstructure, and this
is the main reason for their high susceptibility to localized corrosion such as pitting and
stress corrosion cracking [3–8]. Localized corrosion in aluminium alloys uses to be caused
by microgalvanic effects between IMCs and the matrix [7–10]. This generally results in
pitting corrosion, which is considered to be one of the main microstructure dependent
damage mechanisms of high strength aluminium alloys [7]. Particles constituted by the
alloying elements present different electrochemical activity from the matrix and, therefore,
represent preferential sites for pitting nucleation. In potential-controlled conditions, pitting
is characterized by two types of events, metastable and stable, which occur before and after
the pitting potential, respectively [11].
https://www.mdpi.com/journal/metals
Metals 2021, 11, 980 2 of 14

According to Birbilis and Buchheit [12], three main types of IMCs particles can be
found in high strength Al alloys: precipitates, dispersoids, and constituent particles. The
first ones are formed by nucleation and growth from a supersaturated solution and their
diameters are around few tenths to hundreds of nanometers. They contribute to an increase
in the mechanical resistance of the alloy when they are coherent and homogeneously
dispersed in the matrix [13]. It is reported that they can initiate intergranular corrosion and
stress corrosion cracking when clustered near grain boundaries [12,14,15]. While disper-
soids are typically bigger than the precipitates, they are still within the submicrometric
to micrometric range. Their main role is to control recrystallisation and grain size [12,13].
Since they are mostly passive in environments where Al alloys are usually used and are uni-
formly distributed, they rarely increase corrosion susceptibility [12]. Finally, the constituent
particles, in the present work denominated intermetallics (IMCs), are the largest ones. Its
size range is from a few tenths of a micrometer to up to 10–20 micrometers. They tend to
break down during mechanical treatments [12] and are frequently noticed in clusters [16].
They are enriched in different alloying elements and there is a universal agreement that
pitting corrosion of high strength Al alloys is associated with these particles, mainly in
chloride containing media.
In 2XXX series aluminium alloys, θ’ (Al2 Cu) and S (Al2 CuMg) are two of the most
important types of coarse IMCs particles. The S phase is associated with pitting nucle-
ation [17] and some mechanisms have been proposed in the literature [18]. According
to Moreto, et al. [19] the AA2524-T3 aluminium alloy presents two types of coarse inter-
metallics particles (Al-Cu-Fe-Mn) and incoherent S (Al2 CuMg) precipitates, which are also
found in AA2024-T3 alloys [9,20]. The corrosion behaviour of these intermetallic particles
has been largely investigated in the literature [17,21–27]. The effect of coarse Al-Cu-Mg
IMCs on the localized corrosion behaviour of the AA2024-T3 alloy has been investigated
by Buchheit, et al. [17] and Zhu, et al. [28]. Both authors [17,28] have noticed that this
phase is an anodic site, favouring pitting nucleation. According to the literature [17,24],
at an initial stage, anodic dissolution occurs on S phase particles. During this period,
the Mg is preferentially oxidized, resulting in Cu-rich remnants. This leads to potential
change into the nobler direction, promoting anodic dissolution of the alloy matrix at its
neighbouring boundary. Zhu, et al. [28] proposed a “cathodic corrosion” mechanism to
explain the localized corrosion in 2XXX alloys, which was in disagreement with Buchheit’s
proposal [17]. According to Zhu, et al. [28], during the anodic reaction of S phase particles,
cathodic reactions of water and/or oxygen reduction occur at the neighbouring sites of
the matrix, generating hydroxyl ions (OH− ) [28]. Accordingly, local alkalization occurs
around the S phase remnant and, once the local pH exceeds 9, chemical dissolution of the
surrounding aluminium oxide layer takes place. Subsequently, the bare aluminium matrix
would be oxidized to form a new oxide layer. On the other hand, the Al-Cu-Fe-Mn IMCs
are usually cathodic sites, which are more stable and have less effect on the AA2024-T3
alloy’s corrosion resistance than the Al-Cu-Mg ones [25,29–32].
Very few studies can be found concerning AA2524 [4,33–37], and only a few studies
compare this alloy to the AA2024, focusing on its mechanical properties [2,38]. Although
it is generally accepted that the localized corrosion caused by the IMCs is the nucleation
site for other types of corrosion in high strength Al alloys [23,24], the role of the IMCs on
these alloys’ corrosion initiation has not been well established yet. This is mainly due to
their small size, their chemical and microstructural complexity, and the dependence of
reactivity to the environment [24]. This paper aims to evaluate the corrosion resistances
of both AA2024 and AA2524, to compare the results, and to correlate them with their
microstructure.

2. Materials and Methods

The materials studied in this work were the AA2524-T3 and the AA2024-T3 alloys
produced by ALCOA, both provided as 1.6 mm sheets. Their chemical compositions are
shown in Table 1 and their main mechanical and corrosion properties are shown in Table 2.
Metals 2021, 11, 980 3 of 14

The AA2524-T3 alloy has lower amounts of Fe and Si, which are considered as deleterious
to the corrosion resistance, and a narrower range for the main alloying elements Cu
and Mg [32].

Table 1. Analyzed and nominal chemical composition (wt %) of the AA2024-T3 and AA2524-T3
alloys [39].

Elements AA2024-T3 AA2524-T3

Cu 4.06 (3.8–4.9) 3.84 (4.0–4.5)
Mg 1.77 (1.2–1.8) 1.31 (1.2–1.6)
Mn 0.63 (0.3–0.9) 0.56 (0.45–0.7)
Si 0.11 (0.5 max) 0.04 (0.06 max)
Fe 0.14 (0.5 max) 0.06 (0.12 max)
Ti −(0.15 max) 0.029 (0.10 max)
Zn 0.02 (0.25 max) 0.01 (0.15 máx)
Al Balance Balance

Table 2. Mechanical and corrosion properties of the AA2024-T3 and AA2524-T3 alloys.

Tensile Yield Electrical Open Circuit

Elongation
Strength Strength Conductivity % Potential
(%)
(MPa) (MPa) IACS (VSCE )
AA2024 [40] 435 290 10–15 30 −0.722 [41]
AA2524 [42] 445.4 340.3 19 34 −0.590 [43]

Samples of 400 mm2 were cut from the sheets. Their surfaces were prepared by
grinding them with silicon carbide paper up to # 4000, followed by polishing with a
diamond paste (up to 0.25 µm) to a mirror surface, degreasing in ethyl alcohol, washing
with deionized water, and drying under a hot air stream. The corrosion resistance of both
aluminium alloys was monitored in 0.01 mol L−1 NaCl as a function of exposure time by
immersion tests and electrochemical impedance spectroscopy (EIS).
Experiments were performed using a Solartron 1287 electrochemical interface coupled
to a Solartron 1260 frequency response analyser (FRA), which was used to obtain the elec-
trochemical impedance spectroscopy (EIS) diagrams. The perturbation range was 20 mV
(rms). The acquisition rate was 10 points per decade in a frequency range from 10 mHz to
100 kHz for all samples. The electrochemical tests were performed using a three-electrode
setup configuration with the aluminium alloys as working electrodes and an exposed
area of 1.0 cm2 (Figure 1). The reference electrode used was an Ag/AgCl, 3 mol L−1 KCl,
and a platinum wire was employed as an auxiliary electrode. The electrochemical experi-
ments were carried out in naturally aerated solution at room temperature. Each test was
performed six times to ensure their reproducibility.
The microstructures of the aluminium alloys were analyzed by a Field Emission
Gun Scanning Electron Microscope FEI Quanta 650 (FEG–SEM) prior and after different
exposure periods to the test electrolyte.
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(a) (b)

Figure 1. (a)
Figure Specimen
1. (a) of AA2524
Specimen in as-received
of AA2524 condition
in as-received andand
condition (b)(b)
three-electrode setup
three-electrode configuration
setup cell.cell.
configuration TheThe
reference
reference
electrode (RE) was an Ag/AgCl, 3 mol L−1 KCl, and a platinum wire was employed as an auxiliary electrode (EC). The
− 1
electrode (RE) was an Ag/AgCl, 3 mol L KCl, and a platinum wire was employed as an auxiliary electrode (EC). The
sample was the working electrode (WE).
sample was the working electrode (WE).

3. The microstructures
Results and Discussion of the aluminium alloys were analyzed by a Field Emission Gun
Scanning Electron Microscope FEI Quanta 650 (FEG–SEM) prior and after different expo-
The surface of both the AA2024-T3 and AA2524-T3 alloys were observed by SEM after
sure periods to the test electrolyte.−1
2 h exposure to the 0.01 mol.L NaCl solution. A general view of the microstructures
of the AA2024-T3 and AA2524-T3 alloys are shown in Figure 2a,b, respectively (both
3. Results and Discussion
in an as-received condition). The two main types of coarse IMCs particles (Al-Cu-Mg
The surface
(Figure 2c,d) andof both the AA2024-T3
Al-Cu-Mn-Fe-(Si) and AA2524-T3
(Figure alloys were
2e,f)) were identified observed
by EDX, and bytheySEM
are in
after 2 h exposure
agreement withtothethe 0.01 mol.L
literature −1 NaClHowever,
[9,10,19]. solution. in
A general view ofalloy,
the AA2524-T3 the microstructures
the Al-Cu-Mn-Fe-
of the
(Si) AA2024-T3
particles wereand AA2524-T3
present alloys
in a lower are shown
amount in Figure
and with 2a,b,morphologies
different respectively from
(boththose
in
an found
as-received
in thecondition).
AA2024-T3 The twowhereas
alloy, main types theofAl-Cu-Mg
coarse IMCsareparticles (Al-Cu-Mg
more numerous, (Figure
smaller, and
2c,d) and Al-Cu-Mn-Fe-(Si) (Figure 2e,f)) were identified by EDX, and
more uniformly distributed. The AA2024-T3 alloy is characterized by a smaller number they are in agree-
ment with the
of IMCs, literature
which, [9,10,19].
however, However, larger
are generally in the AA2524-T3 alloy, the
than those found Al-Cu-Mn-Fe-(Si)
in the AA2024-T3 alloy
particles
(Figurewere present in a lower
3). Consequently, amount
the area and of
fraction with
the different
AA2024-T3 morphologies from than
IMC’s is higher thosethe
found in the AA2024-T3
AA2524-T3 (Table 3). alloy, whereas the Al-Cu-Mg are more numerous, smaller, and
more uniformly distributed. The AA2024-T3 alloy is characterized by a smaller number
Comparison
Table 3.which,
of IMCs, of IMCs
however, arearea fractionlarger
generally of AA2024
thanand AA2524
those found alloys.
in the AA2024-T3 alloy
(Figure 3). Consequently, the area fraction of the AA2024-T3 IMC’s is higher than the
Material IMCs Area Fraction (%)
AA2524-T3 (Table 3).
AA2024-T3 2.52 ± 0.42
AA2524-T3 1.64 ± 0.14

The general analysis of the micrographs (Figure 4) show that the corrosive attack is
more evenly distributed on the AA2524-T3 alloy (Figure 4b), whereas for the AA2024-T3
alloy (Figure 4a) it is mainly concentrated around larger IMCs, including the dark areas
around the bigger Al-Cu-Mg precipitates (indicated by arrows). On both alloys, the Al-
Cu-Mn-Fe precipitates showed a rather random behaviour with some of them remaining
intact after 2 h of immersion, likely due to a protective oxide film that hinder the cathodic
reaction, as suggested by Birbilis, et al. [12] (Figure 4a,b).
After 7 h of testing of the AA2024-T3 alloy, the corrosive attack was mainly concen-
trated at the interface between the matrix and the larger intermetallic particles. No localized
corrosion at the grain boundaries was detected. (Figure 4c). Figure 4d shows that most of
the smaller precipitates had been removed from the surface of the AA2524-T3 sample by
the corrosive attack, resulting in a “cleaner” surface in comparison with 2 h of test, even
though some local activity remained around large IMCs. On the other hand, the corrosive
attack of the AA2024-T3 continued to be mainly concentrated at the interface between
Metals 2021, 11, 980 5 of 14

the matrix and the larger intermetallic particles (Figure 4c), which, as previously showed,
were more numerous in this material. For longer immersion times the “cleaning” effect on
Metals 2021, 11, x FOR PEER REVIEW 5 of 15
the AA2524-T3 surface is even more pronounced than that of the AA2024-T3 (Figure 4f,e,
respectively).

AA2024-T3 AA2524-T3
(a) (b)

(c) (d)

(e) (f)

2. Microstructures
Figure 2. MicrostructuresofofAA2024-T3:
AA2024-T3:(a)
(a)general
general view;
view; (c)(c) Al-Cu-Mg;
Al-Cu-Mg; andand
(e) (e) Al-Cu-Mn-Fe-(Si)
Al-Cu-Mn-Fe-(Si) particles.
particles. Microstruc-
Microstructures
tures
of of AA2524-T3:
AA2524-T3: (b) general
(b) general view;view; (d) Al-Cu-Mg;
(d) Al-Cu-Mg; and (f)and (f) Al-Cu-Mn-Fe-(Si)
Al-Cu-Mn-Fe-(Si) particles.
particles. As-received
As-received condition.
condition. SEM–BSE.
SEM–BSE.

After 11 h of exposure to the test electrolyte, most of the small precipitates were
removed from the surface of both alloys (Figure 4e,f). Additionally, Figure 4g,h show the
selective attack near the IMCs for longer exposure periods.
The results showed that IMCs’ area fraction of the AA2524-T3 is lower in comparison
with the AA2024-T3. More than 94% of these IMCs of the first alloy are smaller than 10 µm,
and only 82% of the latter, confirming the theory that the corrosion attack on the AA2524-T3
alloy surface was faster due to its larger number of small particles.
Metals 2021, 11, 980 6 of 14
Metals 2021, 11, x FOR PEER REVIEW 6 of 15

Figure
Figure3.3.Frequency
Frequency(%)
(%)and
andsize distribution
size (µm
distribution
2) of
(µm 2 ) IMCs for for
of IMCs as-received samples.
as-received MoreMore
samples. than 94%
thanof theof
94% AA2524-T3
the AA2524-T3
alloy and 82% of the AA2024-T3 alloy IMCs are smaller than 10 µm2. 2
alloy and 82% of the AA2024-T3 alloy IMCs are smaller than 10 µm .
Table 3. Comparison of IMCs area fraction of AA2024 and AA2524 alloys.
The corrosion resistance of both alloys was also evaluated by EIS with immersion
time and the results are shown in Figures 5 and
Material IMCs6. ItArea
is clearly seen
Fraction (%)that the impedance
modulus associated
AA2024-T3 with the AA2524-T3 alloy was higher than
2.52 ± 0.42 that of the AA2024-T3
during theAA2524-T3
whole test period. Independently of the alloy brand,
1.64 ± 0.14 EIS diagrams are charac-
terized by a broad high frequency depressed capacitive loop followed by a low frequency
capacitive loopanalysis
The general that evolves
of theto a diffusion-controlled
micrographs process
(Figure 4) show thatafter 11 h of exposure
the corrosive attack is to the
test evenly
more electrolyte.
distributed on the AA2524-T3 alloy (Figure 4b), whereas for the AA2024-T3
The EIS
alloy (Figure 4a)results for both
it is mainly alloys were
concentrated fittedlarger
around with the two/three-time
IMCs, including the constants
dark areasequiv-
alent electric
around the biggercircuits (EEC)precipitates
Al-Cu-Mg shown in Figure 7. These
(indicated ECC have
by arrows). beenalloys,
On both established
the Al- in the
literatureprecipitates
Cu-Mn-Fe on aluminium alloys
showed EIS fittings
a rather randomand were also
behaviour withtested
some in
of previous works from
them remaining
our research group [9,44–46]. Table 4 presents the parameters obtained from
intact after 2 h of immersion, likely due to a protective oxide film that hinder the cathodic the equivalent
electrical circuit fitted to the AA2024-T3 and AA2524-T3
reaction, as suggested by Birbilis, et al. [12] (Figure 4a,b). EIS data. The EEC of Figure 7a
was used to fit the data acquired from the first hour until 9 h of immersion, whereas the
diagrams obtained from 11 h until the end of the test were fitted with the EEC of Figure 7b.
In this latter case, the low frequency R//CPE element was substituted for a single CPE,
meant to simulate a diffusion-controlled process. According to Campestrini, et al. [47],
when the resistance associated with the diffusion becomes very large the R//CPE element
may be replaced by a simple CPE element with the exponent “α” value of 0.5, which, in
an ideal situation, is represented by a Warburg element. In the proposed circuits the pair
Rox //CPEox stands for the capacitance of the oxide film in parallel with conductive path-
ways associated with defective sites created by the IMCs, which leads to the unprotected
metal surface. Rct //CPEdl refers to the charge transfer resistance coupled to the charging
of the double layer, whereas CPEcor //Rcor is ascribed to the low frequency corrosion
processes that kinetically control the alloys’ deterioration, which gradually evolves to a
diffusion-controlled process and is likely associated with the oxygen reduction reaction
taking place in nobler IMCs.
Metals 2021, 11, 980 7 of 14
Metals 2021, 11, x FOR PEER REVIEW 7 of 15

AA2024-T3 AA2524-T3

(a) (b)
2h

(c) (d)
7h

(e) (f)
11 h

(g) (h)
20 h

Figure4.4.Microstructures
Figure MicrostructuresofofAA2024-T3
AA2024-T3after
after(a)
(a)22h,h,(c)
(c)77h,h,(e)
(e)11
11h,h,and
and(g)
(g)20
20h.h.AA2524-T3
AA2524-T3after
after(b)
(b)22h,h,(d)
(d)77h,h,(f)
(f)11
11h,h,
and (h) 20 h of exposure to the 0.01 mol.L
− −1
1 NaCl solution. SEM–BSE. The micrographs show the evolution
and (h) 20 h of exposure to the 0.01 mol.L NaCl solution. SEM–BSE. The micrographs show the evolution of the localized of the localized
corrosion at the interface IMC/matrix (indicated by arrows).
corrosion at the interface IMC/matrix (indicated by arrows).

After 7 h of testing of the AA2024-T3 alloy, the corrosive attack was mainly concen-
trated at the interface between the matrix and the larger intermetallic particles. No local-
ized corrosion at the grain boundaries was detected. (Figure 4c). Figure 4d shows that
most of the smaller precipitates had been removed from the surface of the AA2524-T3
 Metals2021,
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2021,11, FOR PEER REVIEW 8 of 149 of 15

Bode Phase Angle Nyquist

Figure 5. Evolution of EIS results for the AA2024-T3 as a function time of exposure to 0.01 mol L−1 NaCl electrolyte.
(A) Bode phase angle and (B) Nyquist diagram. Measurements were taken after 2, 5, 7 and 9 h of the experiment. (C) Bode
Figure 5. Evolution of EIS results for the AA2024-T3 as a function time of exposure to 0.01 mol L−1 NaCl electrolyte. (A)
phasephase
Bode angle angle
and (D) Nyquist
and diagram.
(B) Nyquist Measurements
diagram. were taken
Measurements wereafter 11, 20,
taken 48 and
after 2, 5,72 h of the
7 and 9 h experiment.
of the experiment. (C) Bode
phase angle and (D) Nyquist diagram. Measurements were taken after 11, 20, 48 and 72 h of the experiment.
Table 4 shows the evolution of the Rox //CPEox values. For both alloys, CPEox increased
with exposure time. SEM analysis has shown that as the corrosive attack proceeded,
holes were formed in the samples surface as a result of the dissolution/detachment of the
IMCs particles increasing the effective area exposed to the electrolyte [10]. If pits did not
progress in these regions, a fresh oxide layer was formed. However, it should be more
defective. Both facts contribute to capacitance increase. In addition, from the beginning
of the exposure period, and during the whole test, CPEox was smaller for AA2524-T3,
indicating the presence of a thicker oxide layer in this alloy, in agreement with the results
from previous studies in the literature [46,48].
Metals
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Bode Phase Angle Nyquist

Figure 6. Evolution of EIS results for the AA2524-T3 as a function time of exposure to 0.01 mol −1 L−1 NaCl electrolyte.
Figure 6. Evolution of EIS results for the AA2524-T3 as a function time of exposure to 0.01 mol L NaCl electrolyte. (A)
(A) Bode phase angle and (B) Nyquist diagram. Measurements taken after 2, 5, 7, and 9 h of the experiment. (C) Bode phase
Bode phase angle and (B) Nyquist diagram. Measurements taken after 2, 5, 7, and 9 h of the experiment. (C) Bode phase
angle
angleand
and(D)
(D)Nyquist
Nyquistdiagram.
diagram.Measurements
Measurementstaken
takenafter
after11,
11,20,
20,48,
48,and
and7272h hofofthe experiment.
the experiment.

Concerning Rox , Table 4, it also increased with immersion time, indicating that electro-
The EIS results for both alloys were fitted with the two/three-time constants equiva-
chemically active sites on both alloys’ surfaces become less numerous and/or were less
lent electric circuits (EEC) shown in Figure 7. These ECC have been established in the
easily reachable. As already demonstrated in the SEM analysis (Figure 4), the selective
literature on aluminium alloys EIS fittings and were also tested in previous works from
attack near the IMCs results in surface “cleaning”, leading to a lower number of active
our research group [9,44–46]. Table 4 presents the parameters obtained from the equiva-
sites. In addition, deposition of corrosion products was frequently found above large IMCs.
lent electrical circuit fitted to the AA2024-T3 and AA2524-T3 EIS data. The EEC of Figure
These features would hinder the access of aggressive species to the matrix surface and can
7a was used to fit the data acquired from the first hour until 9 h of immersion, whereas
contribute to the Rox increase. Accordingly, as the surface of AA2524-T3 progressively be-
the diagrams obtained from 11 h until the end of the test were fitted with the EEC of Figure
came “cleaner” than AA2024-T3, the rate of the Rox increase was much faster for the former
7b. In this latter case, the low frequency R//CPE element was substituted for a single CPE,
alloy. Therefore, it is proposed that the attack of the small particles and their removal from
meant to simulate
surface are the mainareasons
diffusion-controlled process.
for the Rox increase, as According
this reducestothe
Campestrini, et al. [47],
number of defective
sites where electrochemical reactions could take place. However, blocking of active element
when the resistance associated with the diffusion becomes very large the R//CPE site by
may be replaced
aluminium by aprecipitation
hydroxide simple CPE element
may alsowith
havethe exponent to
contributed “α”thevalue of 0.5, which, in
Rox increase.
an ideal situation, is represented by a Warburg element. In the proposed circuits the pair
Rox//CPEox stands for the capacitance of the oxide film in parallel with conductive path-
ways associated with defective sites created by the IMCs, which leads to the unprotected
metal surface. Rct//CPEdl refers to the charge transfer resistance coupled to the charging of
the double layer, whereas CPEcor//Rcor is ascribed to the low frequency corrosion processes
 Metals 2021, 11, x FOR PEER REVIEW 11 of 15

Metals 2021, 11, 980 that kinetically control the alloys’ deterioration, which gradually evolves to a diffusion-
10 of 14
controlled process and is likely associated with the oxygen reduction reaction taking place
in nobler IMCs.

(a)

(b)

Figure 7. Equivalent electrical circuits (EEC) proposed to fit the data of the AA2024-T3 and AA2524-
Figure
T3 7. Equivalent
(a) until 9 h and (b)electrical
from 11 circuits (EEC) proposed
h of immersion in a 0.01to fit L
mol −1data
the NaClofsolution.
the AA2024-T3 and AA2524-
T3 (a) until 9 h and (b) from 11 h of immersion in a 0.01 mol L−1 NaCl solution.
As mentioned earlier, the Rct //CPEdl pair is associated with the charge transfer reac-
tions from
Table 4. Parameters obtained (Rct ) the
occurring at the
equivalent interface
electrical offitted
circuit the matrix at the defective
to the AA2024-T3 sites of the
and AA2524-T3 EISoxide
data. (near
active IMCs). The evolution for the components Rct and CPEdl with exposure time to
2h 5h 7h 9h 11 h 20 h 48 h 72 h
the 0.01 mol L−1 NaCl electrolyte is shown in Table 4. For AA2524-T3, Rct behaviour
2524 2024 2524 was2024 2524 2024
significantly 2524 during
oscillating 2024 the 2524whole2024 2524 2024
immersion period, 2524
which 2024
must2524 2024a
has been
Rsol consequence of 382.80
the detachment and328.40
outbreak of new IMCs as 316.90
corrosion proceeded. For
346.40 394.20 342.10 388.70 334.90 330 380.40 381.20 325.10 373.80 362.30 318.80 376.90
Ω·cm2 this sample, CPEdl remained almost constant during the first 15 h, indicating that the
Error (%) 0.40 0.27 0.50electrochemically
0.22 0.40 0.16 active0.32
surface0.16
area0.34
remained0.27 almost
0.34 unchanged.
0.25 0.37 However,
0.37 0.32 from0.30
this
CPEox period onwards the decrease in CPEdl might be attributed to the formation of corrosion
µF·cm−2·s( 6.27 16.60 5.99products
16.30 on some
6.07 active6.39
14.90 areas,15.30
clearly6.84
indicated
19.20on8.58
the AA2524-T3
20.80 13.80 surface,
34.70 that partially
18.00 43.30
α−1) blocked these sites.
Error (%) 2.44 8.14 2.36 5.84 Conversely,
1.75 3.88for AA2024-T3,
1.28 3.52after1.29 up to4.57
40 h of1.27 3.41Rct 1.39
testing, decreased
4.28 continuously.
1.44 3.63
This tendency may be explained by the enrichment in the more noble components of the
Rox
327.10 57.15 351.60 56.04 413.10
remaining active57.71
IMCs.479.10 64.06 even
Therefore, 541.80though
79.83 in
752.30
smaller107number,
954.50due210.20 761.40 239.70
to detachment,
Ω·cm2
enhanced galvanic activity would be expected between the matrix and the Cu-enriched
Error (%) 6.18 9.32 4.53IMCs.5.17 For3.78
longer 3.02 3.15 2.77
immersion 3.37an 3.78
periods, increase5.21
of R3.33 7.58 9.46 7.78 10.02
ct was observed. This can be
CPEdl ascribed to the precipitation of corrosion products above the IMCs and their vicinity,
µF·cm−2·s( 14.80 58.90 16.40 75.40
which 16.60 89.30
provided 16.10
a barrier 91.50 the
between 14.40 83.50 11.50
electrolyte and the 80.80 8.85surface.
metallic 44.00 Accordingly,
13.10 50.20
α−1)
CPEdl initially increased, indicating that the electrochemically active surface augmented.
Error (%) 3.23 3.39 3.26However, for longer
2.19 3.13 1.40 exposure
2.53 1.35 times,2.84
it started
2.06 to4.65
decrease
2.14 due to active
6.20 6.93 surface area
4.73 6.19
α dl 0.86 reduction as corrosion products precipitated.
0.89 0.88 0.88 0.88 0.87 0.87 0.87 0.89 0.89 0.90 0.90 0.97 0.99 0.94 0.96
Error (%) 0.81 0.66 0.81 0.49 Finally, the low
0.83 0.35frequency
0.71 0.36time constant,
0.78 0.50 corresponding
1.33 0.57 to 1.74the rate-controlling
1.79 1.40 1.69 step
Rct of the corrosion process, was mainly represented by CPEcor and its “αcor ”, and Rcor were
7.37 4.66 7.73important
4.37 6.98
only up 4.28 7.27hours
to nine 4.06of exposure.
7.88 3.16During 6.26 the3.48
initial5.43 2.47 period,
immersion 6.54 3.50αcor
kΩ·cm2
values ranged between 0.69 and 0.83, suggesting a mixed controlled process for both
Error (%) 2.09 2.94 2.89 2.78 2.61 2.20 2.01 2.11 2.88 2.61 3.79 3.43 4.30 5.09 3.03 5.48
alloys, corresponding to the period where the EIS diagrams were fitted with the EEC of
CPEcor Figure 6. For longer immersion times, “αcor ” varied between 0.4 and 0.6, showing the main
µF·cm−2·s( 174.00 180.04 187.70 241.00 239.59
contribution 313.00 274.00
of diffusive 358.00likely
processes 204.00 341.00 283.00
through 327.00 199.00
the precipitated 352.41products.
corrosion 275.00 295.00
α−1)
Higher capacitance values were associated with the AA2024-T3 alloy comparatively
Error (%) 1.95 1.00 3.31to the
1.28 3.05 1.38
AA2524-T3 (Table2.88 1.44
4) after 3.07 hour
the first 1.16of immersion,
4.46 1.87 although
2.65 1.75 there2.71 1.98
was much
α cor 0.76 larger variation in the CPE values for this latter alloy,
0.81 0.63 0.74 0.65 0.69 0.64cor 0.64 0.45 0.54 0.46 0.50 0.42 0.59 0.57 0.60 likely due to the stronger con-
Error (%) 1.77 1.00 2.78tribution
1.42 of3.26
partially
1.51 soluble
2.72 corrosion
1.43 2.25 products
0.79 on3.84
active1.26
sites at its surface
1.70 1.33 which
2.16 were
1.56
periodically removed.
The electrochemical results demonstrated that the corrosion resistance of the AA2524-
T3 was higher than the AA2024-T3.
Metals 2021, 11, 980 11 of 14

Table 4. Parameters obtained from the equivalent electrical circuit fitted to the AA2024-T3 and AA2524-T3 EIS data.

2h 5h 7h 9h 11 h 20 h 48 h 72 h
2524 2024 2524 2024 2524 2024 2524 2024 2524 2024 2524 2024 2524 2024 2524 2024
Rsol Ω·cm2 346.40 394.20 342.10 388.70 334.90 382.80 330 380.40 328.40 381.20 325.10 373.80 316.90 362.30 318.80 376.90
Error (%) 0.40 0.27 0.50 0.22 0.40 0.16 0.32 0.16 0.34 0.27 0.34 0.25 0.37 0.37 0.32 0.30
CPEox
6.27 16.60 5.99 16.30 6.07 14.90 6.39 15.30 6.84 19.20 8.58 20.80 13.80 34.70 18.00 43.30
µF·cm−2 ·s(α−1)
Error (%) 2.44 8.14 2.36 5.84 1.75 3.88 1.28 3.52 1.29 4.57 1.27 3.41 1.39 4.28 1.44 3.63
Rox Ω·cm2 327.10 57.15 351.60 56.04 413.10 57.71 479.10 64.06 541.80 79.83 752.30 107 954.50 210.20 761.40 239.70
Error (%) 6.18 9.32 4.53 5.17 3.78 3.02 3.15 2.77 3.37 3.78 5.21 3.33 7.58 9.46 7.78 10.02
CPEdL
14.80 58.90 16.40 75.40 16.60 89.30 16.10 91.50 14.40 83.50 11.50 80.80 8.85 44.00 13.10 50.20
µF·cm−2 ·s(α−1)
Error (%) 3.23 3.39 3.26 2.19 3.13 1.40 2.53 1.35 2.84 2.06 4.65 2.14 6.20 6.93 4.73 6.19
α dL 0.86 0.89 0.88 0.88 0.88 0.87 0.87 0.87 0.89 0.89 0.90 0.90 0.97 0.99 0.94 0.96
Error (%) 0.81 0.66 0.81 0.49 0.83 0.35 0.71 0.36 0.78 0.50 1.33 0.57 1.74 1.79 1.40 1.69
Rct kΩ·cm2 7.37 4.66 7.73 4.37 6.98 4.28 7.27 4.06 7.88 3.16 6.26 3.48 5.43 2.47 6.54 3.50
Error (%) 2.09 2.94 2.89 2.78 2.61 2.20 2.01 2.11 2.88 2.61 3.79 3.43 4.30 5.09 3.03 5.48
CPEcor
174.00 180.04 187.70 241.00 239.59 313.00 274.00 358.00 204.00 341.00 283.00 327.00 199.00 352.41 275.00 295.00
µF·cm−2 ·s(α −1)
Error (%) 1.95 1.00 3.31 1.28 3.05 1.38 2.88 1.44 3.07 1.16 4.46 1.87 2.65 1.75 2.71 1.98
α cor 0.76 0.81 0.63 0.74 0.65 0.69 0.64 0.64 0.45 0.54 0.46 0.50 0.42 0.59 0.57 0.60
Error (%) 1.77 1.00 2.78 1.42 3.26 1.51 2.72 1.43 2.25 0.79 3.84 1.26 1.70 1.33 2.16 1.56
Rcor kΩ·cm2 22.46 30.15 27.51 27.98 27.91 33.66 26.06 54.26
Error (%) 3.36 1.93 5.35 3.70 8.76 5.49 6.94 7.53
Metals 2021, 11, 980 12 of 14

4. Conclusions
In this study, the corrosion resistances of the AA2024-T3 and the AA2524-T3 alloys
were compared. The differences between these alloys are the number and the precipitates’
area fraction. The AA2024-T3 alloy has a smaller number of IMCs, which, however, are
larger than those found in the AA2524-T3 alloy. Therefore, the IMCs area fraction of the
former is higher than the latter. The SEM results suggest that the rapid removal of active
sites from the AA2524-T3 surface (smaller IMCs) promotes a cleaner surface.
The hypothesis that defective areas prone to electrochemical reactions were removed
from AA2524-T3 was confirmed by the EEC fitting to EIS results, as AA2524 Rox increases
and CPEox decreases with immersion time. Additionally, the corrosion process of AA2524,
represented by CPEcor , “αcor ” and Rcor , are significant only up to nine hours of exposure
and confirm the higher contribution of active sites of the surface, caused by partially soluble
corrosion products.
The electrochemical tests also showed that the localized corrosion resistance of the
AA2524-T3 was higher than the AA2024-T3 during the whole test period. This was
indicated by the higher impedance values associated with the first alloy and confirmed by
surface observation after various immersion periods in the tested electrolyte. On the other
hand, SEM analysis showed that the corrosion attack on the AA2524-T3 alloy surface was
faster due to its larger number of small particles.

Author Contributions: Conceptualization, I.C. and H.G.d.M.; methodology, F.M.Q. and M.T.; valida-
tion, I.C. and H.G.d.M.; formal analysis, F.M.Q. and M.T.; investigation, F.M.Q., M.T. and A.F.S.B.;
writing—original draft preparation, M.T. and A.F.S.B.; writing—review and editing, M.T. and A.F.S.B.;
visualization, I.C. and H.G.d.M.; supervision, I.C.; project administration, I.C.; funding acquisition,
I.C. All authors have read and agreed to the published version of the manuscript.
Funding: This research was funded by CNPq, grants number 400895/2014-5, 400781/2013-1 and
158764/2014-5 and CAPES, grant number 1536157.
Data Availability Statement: Not applicable.
Acknowledgments: The authors acknowledge CNPq and CAPES.
Conflicts of Interest: The authors declare no conflict of interest.

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